Process for the fractional separation of paraffin and like substances and of mixtures of such substances with oil.



PROCESS EGR THE FRACTEONAL SEPARATION OF PARAFFIN ANI) LIKE SUBSTANCES AND QF Il XTUEES O?? SUCH SUBSTANCES "WXTH OIL.

l Application tiled February 7. v1912. Serial No. 678,137.

To all whom may concern Be it known that l, KARL Urn. working director, residing at St. Maria Maddalena lnferiore 1285, Trieste. Austria-Hungary, have invented certain new and useful improvements in a Process for the Fracticnal Separation of Paratiin and Like Substances and of Mixtures of Such Substances with Oil, of which the following is a specitication.

The modern process for producing paraflins used by nearly all manufacturers,.con sists in the 'three following steps: l. tallizing the paratlins by cooling the distillate containing paraffin and separating the crystals obtained from the oil by filtering in tiltcr presses. 2. Improving the paraiiins which come out of the filter presses and still contain a large amount of oil, (parn-o'utter). 3. Finally extractingr the oil from the improved parain-butter by the schwitz or sweating process.

The object of the present invention is to provide a process for carrying out all the improved processes in such a manner as to cut down the amount of work necessary to a minimum; and to provide a simple cheap and economic method of doing the same. lnstead of allowing a smooth mass to form, as has heretofore been the case, ,having soft crystals, l which the parathn crystals could be separated only by means oi a filter press or other expensive apparatus, the present process accomplishes the separation of the solid. from the liquid materials without other .means than a crystallizer in which the paraffin will crystallize upon the cooling of the material therein.

rlrials have shown that on following determined rules of operation the i parallin crystals melting at a higher temperature can be separated shortly. after their production from the paraflin-hutter in they precipitate entirely from the still liquid part in order to solidify on the bottom of the vessel into a solid feltlike mass through which the liquid portions can easily percolate and that only a minimum ol' oil adheres to the crystals obtained in this manner. For the realization of this action the following are essential: l. The absolute rest ory quietude of the individual particles of parafn. The rapidity of cooling down. 3. rThe Specication of Letters Patent.

Cryscapable of being poured, and froml such manner that Patented Feb. iid, 19H37..

blades c therein with any means for rotating them extremely slowly. At their vertical edges. these blades are provided with scrapers c to prevent the contents from sticking' to the sides of the retainer. At the bottom of the retainer is a. sieve c of fine wire mesh which acts as a support for the` felt like mass of crystallized para-itin and enahles the fluid to be drawn oihfleaving he- 'hind the mass. though the conical shaped bottom and the valve d.

Means for cooling the contents o' the container a are provided consisting of a channel f encircling the container and secured thereto near the top edge, having a series ot' small perforations h in the bottom thereof. The lower end of the container is encircled and has secured thereto a somewhat' similar chiinnel g but without' perforations. A pipe (Fig. 3) is provided to supply the channel f with water or other cooling liquid. ln operation the cooling water from the pipe flows in'to and around in thechannel when by means of the perforations k 1t trickles therefrom and down the side of the container a until it is caught by the channel f3 and conducted away.

The operation of my invention is as follows: Paraiiin-butter is first heated to 42 C.,

or 2 C. above its melting point, and then introduced into the retainer. The blades are then caused to rotate very slowly--so slowly that the entire mass is moved as a unit and no relative or mutual change whatever takes place between the particles, as this rotation is for the sole purpose oi' facilitating the-cooling of the mass and not any disarrangement of the paraffin particles. Subsequent to this rotation, the cooling device is set in operation and arranged to cool ythe mass 0.6 to 0.80 C. per hour until the or raisers. essaiera-HUNGARY, Assreuon or ons-Hans" To remeras. MrrrEnaL-onnnarrrnnsrn, or rnrnsrn, Alvernia-HUNGARY.

i' terrine-rature.v vhas been reduced to 29 which will take about 18 hours.,

aofi

i paraffin-butter i process the .liquid have been stopped. For this drawing ol' to 1 hour isrequired. accord- C. The rotatioiiof the blades is continued all through the cooling process to aid in the uniform cooling of the mass. During the cooling, the 4se aration .of the paraiin takes place by theft' imation of crystals having greater specific gravity than the butter which sink to the bottom where they form into a feltlike porous mass. This mass falls upon the sieve where it is supported to allow the soft paraiin and oil'topermeate through it and be drawn off.- After the end ofthe cooling part is left to run out through the porous mass of paraiiin Which is supported by a wire sieve c arranged above the bottom b and through the sieve by means of the valve d secured at the lowest point.

v The condition mentioned under l is fulllled by the slow rotationI of the mass in such a way that the mass is revolved as a vunit with no disarrangement of the paraf- 4fin particles taking place.

he most appropriate speed of rotationv of the blades e when paralin and oil are to be separated is found to be, one revolution per minute, but wheadierent parafns, such as soft and hard, are to be separated, two 'revolutions per-minute is most appropriate. n

he conditions Vmentioned under 2 and 3 are variable according to the melting point i and contents of paralin in thi^ to be treated.

raw material the percolation of the oil takes place in the above mentioned manner after the rotating device and the artificial cooling device percolation or 1n?- to the size of the apparatus. There resu ts then about 40% in weight of the -used as liquid 29' C. and containing. 0%` of which is let run4 into any kind of a container and 60% in weight 'as paraffin mass ceasing to flow at 46-47 C. and containing about-82% of paraiin lwhich means of a` steam-coil in another vessel.

l 'AThe process characterized in the foregoadvantageously deeper vessel.

`parailfin and like At the temperature of 29C oil, solidifying at is melted by i,

1,128,4ee i by means of the above described proc-- vess, the soft paraflins assume the part of the oil. But the cooling down must here take place'much slower. When, for instance, paraffin free from oil ceasing to How at 53 lC. is filled at a temperature of 55 in the;`

same apparatus, cooling in this temperature after the vfirst hour sinks to 53 C., and from then on in each hour 0.2 C. down to a temperature ofj 51 C. The

down takes place time of cooling amounts then to 11 hours,

during which time the harder paraffin takes paraiiin which is then in a liquid state in the upper part vof the apparatus is then peroolated, as described further above, in the same manner through precipitated porous mass of-lia'rd pa-ralins and collected in a It will have 'a temperature when it ceases to flow of 51. The hard paraiiin mass is melted in another vessel and ceases to flow at 55.. The proportion precipitation of the 'or quantityv of soft and hard paraffin is about 1:1.

I claim:

A process for the fractional separation of substances, consisting in rst reducing the material to a molten condition, then simultaneously cooling the substances below the temperature of congelation, and slowly effecting a horizontal displacement of the molten mass as a-whole until the paraffin crystals gradually precipitate at the bottom forming a spongy layer,

and finally filtering the oil and soft paraiiin through said layer, substantially as described.

manner that the I place. The softer lIn testimony whereof I alixmy ,signature in presence of two witnesses.

. KARL OPL.

lVitnesses: p

' ALFRED BARHNAD,

Heo ABBOMONOUGH. 

